HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium aluminum hydride → [5-(3-chloro-benzylamino)-2-methyl-2H-pyrazol-3-yl]-methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium aluminum hydride | HCID 28112 | — |
| Reactant | Sodium sulfate decahydrate | HCID 62649 | — |
| Reactant | 5-(3-chloro-benzylamino)-2-methyl-2H-pyrazole-3-carboxylic acid methyl ester | HCID 57619417 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | [5-(3-chloro-benzylamino)-2-methyl-2H-pyrazol-3-yl]-methanol | HCID 57619232 | — |
Reaction Conditions
| Temperature | -40 °C |
|---|
Reaction Steps
5-(3-Chloro-benzylamino)-2-methyl-2H-pyrazole-3-carboxylic acid methyl ester (646, 0.944 g, 3.37 mmol) was combined with tetrahydrofuran (20 mL) and the solution was cooled to −40° C. 1.0 M lithium tetrahydroaluminate in tetrahydrofuran (3.7 mL) was added and the reaction was stirred for 45 min at −20° C. 1.0 M lithium tetrahydroaluminate in tetrahydrofuran (3.7 mL) was added at −40° C. and the reaction was stirred to 10° C. Sodium sulfate decahydrate was added in small portions and the mixture was stirred for two hours at room temperature, then filtered through Celite and concentrated. The resulting compound (647, 0.821 g, 97%) was washed with a mixture of ethyl acetate:hexanes and dried under reduced pressure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169250B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-83c5e037de624f88b7f00ee92b30f6a6 |
| Source note | uspto-grants-2015_10 |